CN108680655A - A kind of high-throughput Continuous Flow Analysis method of Cr VI in colorized cigarette paper and tipping paper - Google Patents
A kind of high-throughput Continuous Flow Analysis method of Cr VI in colorized cigarette paper and tipping paper Download PDFInfo
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- CN108680655A CN108680655A CN201810146844.5A CN201810146844A CN108680655A CN 108680655 A CN108680655 A CN 108680655A CN 201810146844 A CN201810146844 A CN 201810146844A CN 108680655 A CN108680655 A CN 108680655A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses the high-throughput Continuous Flow Analysis methods of Cr VI in colorized cigarette paper and tipping paper, include the following steps：It weighs 0.20g samples to be placed in 25mL sample cells, then 100 sample feeding pipes is piled to the sample injection disc of Continuous Flow Analysis instrument；B, dipotassium hydrogen phosphate cushioning liquid 20mL is separately added into each sample cell, then it is sequentially inserted into the inner sleeve of the internal filtering sieve plate for having solid phase extraction filler and bottom to carry 0.45 μm of aperture, sample disc is put on oscillator after being plugged inner sleeve, oscillation extraction is carried out by selected oscillation extraction condition；C, the inner sleeve of sample cell is pushed after having extracted, the sample solution extracted is allowed to be entered in inner sleeve by the filtering sieve plate and the solid phase extraction filler, sample disc is placed on the autosampler of Continuous Flow Analysis instrument again, the sample introduction needle of autosampler is only insertd at the supernatant in inner sleeve every time to draw the supernatant by filtering and extracting, and is transferred in Continuous Flow Analysis instrument and is analyzed.
Description
Technical field
The invention belongs to tobacco chemistry research fields, and in particular to the height of Cr VI in a kind of colorized cigarette paper and tipping paper
Flux Continuous Flow Analysis method.
Background technology
With the development of tobacco science and technology, modern printing technology is used widely in cigarette manufacture, especially for volume
Cigarette paper and tipping paper, rational color printing can form strong visual contrast, attract the attention of consumer, enhancing cigarette production
The brand image of product also has certain anti-fake effect.But in printing process, some harmful components also can to some extent by
It is brought into cigarette paper and tipping paper, therefore controls colorized cigarette paper and tipping paper exogenous pollutant to ensureing cigarette product
Safety be of great significance.
Cr VI is exogenous heavy metal contaminants important in colorized cigarette paper and tipping paper, and Cr VI is imbedibility pole
Poisonous substance, skin contact may lead to sensitivity；It is more likely to that inherited genetic defects, sucking is caused to be potentially carcinogenic, has persistently to environment
It is dangerous.The harm of Cr VI at home and abroad attracts wide attention, and content of 6-valence Cr ions in packaging material is made by European Union
It clearly limits the quantity, Cr VI is also determined as one of the toxicant of 17 kinds of highly dangerous by U.S.EPA (EPA).
The detection of Cr VI at present mainly use atomic spectroscopy, liquid chromatogram-inductively coupled plasma mass spectrometry, from
Sub- chromatography, chemoluminescence method, spectrophotometry, connected neighbor set etc..Wherein connected neighbor set has automation
The prominent advantages such as degree is high, analyze speed is fast, reagent dosage and discharging of waste liquid are few, have obtained answering extensively in sexavalence chromium analysis
With.China Tobacco Corporation has issued the company standard (YQ/T using connected neighbor set determination of hexavalent chromium in 2015
60-2015), sample is extracted with buffer solution, extract liquor after Solid Phase Extraction column purification in Flow Analyzer and color developing agent 1,
Two hydrazine on-line mixing of 5- diphenyl phosphinylidyne develops the color, and passes through spectrophotometer detection assay.It, need to be by sample in sample pretreatment process
Product are weighed into ground triangular flask, and extractant oscillation extraction is added, and are filtered, will be filtered with the qualitative filter paper funnel folded in advance
Sample solution afterwards is pipetted to methanol, water and the pretreated polyamide SPE columns of dipotassium hydrogen phosphate solution, waits for that sample flows completely
After going out, dipotassium hydrogen phosphate solution elution polyamide SPE columns are added, merges and collects efflux and leacheate, it then again will be through solid
The test solution of phase extracting and purifying is transferred in the sample feeding pipe of Continuous Flow Analysis instrument, carries out subsequent measurements.As it can be seen that sample pre-treatments mistake
Cheng Zhongxu shifts sample several times；Solid-phase extraction column for purification is using preceding needing to be pre-processed with 3 kinds of solution, sample solution mistake
Elution solid-phase extraction column is also needed after column；Moreover, needing qualitative filter paper being folded into funnel in filtering to filter use.Look forward to mark method
Pre-treatment step is more, cumbersome, detection efficiency is low, and introducing that may be because of impurity in transfer process and extracting solution
It accidentally splashes etc. and to influence the reliability of testing result.
Therefore, there is an urgent need to the analyzing detecting methods of a kind of high-precision for Cr VI and high throughput.
Invention content
The purpose of the present invention is to provide a kind of continuous flowings point of the high throughput of Cr VI in colorized cigarette paper and tipping paper
Analysis method comprising following steps：
A, 0.20g samples accurately are weighed to be placed in 25mL sample cells, is removed from Continuous Flow Analysis instrument autosampler
Sample injection disc will claim excellent sample feeding pipe to be put into successively on Continuous Flow Analysis instrument sample injection disc, until by 100 in the sample injection disc
All pile sample cell in sample cell position；
B, dipotassium hydrogen phosphate cushioning liquid 20mL is separately added into each sample cell with the liquid-transfering gun of 25mL, then successively
It is inserted into the inner sleeve of the internal filtering sieve plate for having solid phase extraction filler and bottom to carry 0.45 μm of aperture, prevents oscillation extraction process
Middle solution splashes out, and sample disc is put on oscillator after being plugged inner sleeve, is carried out by the oscillation extraction condition that standard method is selected
Oscillation extraction；
C, the inner sleeve of sample cell is pushed after having extracted, the sample solution extracted is allowed to pass through the filtering sieve plate and institute
It states solid phase extraction filler to enter in inner sleeve, then sample disc is placed on the autosampler of Continuous Flow Analysis instrument, from
The sample introduction needle of dynamic injector is only insertd into every time to draw the supernatant by filtering and extracting at the supernatant in inner sleeve, is turned
Enter and is analyzed in Continuous Flow Analysis instrument.
Preferably, sealing ring is carried at the top of the sample cell, the inner sleeve is inserted into the sealing before oscillation extraction
In circle, extract liquor is then added, inner sleeve is stuck in the oral area of sample cell prevents extract liquor in oscillatory process from splashing out, but inner sleeve
The filtering sieve plate of bottom is not contacted with sample；Inner sleeve is pushed after sample extraction is complete, extract liquor, which is just filtered by sieve plate, to be entered
Into inner sleeve, autosampler can extract sample directly from inner sleeve and be analyzed.
In order to reduce transfer workload, inventor have also been devised with the matched oscillator of the sample disc of autosampler, can
Sample disc is removed from autosampler, fills direct oscillation extraction after a disk sample, inner sleeve filtering, entire sample after having extracted
Product disk is put on autosampler and is analyzed again.Whole operation flow need not shift specific sample, before sample
Processing procedure is greatly simplified, and sample analysis efficiency is compared with current tobacco business standard method and several times can be improved.And
The reduction of transfer step can effectively prevent the error in sample pre-treatments operating process, greatly reduce the introducing of human error.
In addition, when being measured to the Cr VI in colorized cigarette paper and tipping paper using enterprise's mark method, for purifying sample
For the solid-phase extraction column of product solution using preceding needing to be pre-processed with 3 kinds of solution, sample solution, which is crossed after column, also needs elution Solid Phase Extraction
Column.Solid phase extraction filler HLB stability of the present invention is preferable, and the extraction of sample solution can be directly carried out without activation
It purifies, inner sleeve is depressed after sample extraction can be completed at the same time filtering and the Solid Phase Extraction of sample extracting solution, simplify sample
Product solid phase extraction manipulations flow, greatly improves work efficiency.
When sample analysis, flow analysis operation is carried out by Fig. 3；By 60-2015 (cigarettes of tobacco enterprise standard YQ/T
Paper Determination of Hexavalent Chromium continuous flow method) as defined in condition be measured.The workmanship composition of potassium bichromate standard solution is first used when measurement
Line, sample are placed on autosampler in order, and the titer of an intermediate concentration is put after 10 samples as quality
Control (sample introduction frequency is 1 sample per minute)；Analysis after hours, according to peak height from working curve calculate sample in water
Dissolubility sugared content.
Choose colorized cigarette paper and tipping paper sample, respectively in the present inventive method with tobacco enterprise standard YQ/T60-
2015 (cigarette tipping paper Determination of Hexavalent Chromium continuous flow methods) carry out Determination of Hexavalent Chromium, and are compared (table 1) to result.This
Inventive method measurement result and at present, without significant difference, analysis result accurately may be used with tobacco enterprise standard method measurement result
It leans on.
The comparison of table 1 the method for the present invention and company standard
Beneficial effects of the present invention
For insufficient present in enterprise's mark method, the present invention establishes a kind of Solid Phase Extraction-continuous flow method and quickly measures
The method of Cr VI in colorized cigarette paper and tipping paper, in method of the invention, whole operation flow need not shift sample, from
And sample pretreatment process is made to be greatly simplified.Using more than two sample disc alternate treatments (before a disk sample introduction, a disk
Processing), it continual can be analyzed, daily 2 people can handle 8-10 disk samples, and routinely 60 samples of sample introduction speed/h is calculated, often
It can analyze 400 or more samples, and sample analysis efficiency is compared with current tobacco enterprise standard method and several times can be improved, and
Actual sample analysis result and current company standard method are consistent.
In addition, when being measured to the Cr VI in colorized cigarette paper and tipping paper using enterprise's mark method, for purifying sample
For the solid-phase extraction column of product solution using preceding needing to be pre-processed with 3 kinds of solution, sample solution, which is crossed after column, also needs elution Solid Phase Extraction
Column, solid phase extraction filler HLB stability of the present invention is preferable, and the extraction of sample solution can be directly carried out without activation
It purifies, inner sleeve is depressed after sample extraction can be completed at the same time filtering and the Solid Phase Extraction of sample extracting solution, simplify sample
Product solid phase extraction manipulations flow, greatly improves work efficiency.
Description of the drawings
Fig. 1 is the sample injection disc used in the present invention.
Fig. 2 is the sample feeding pipe used in the present invention and the schematic diagram of inner sleeve.Wherein a figures are sample feeding pipes；B figures are inner sleeves
Pipe；C figures are schematic diagram when inner sleeve is inserted at the top of sample feeding pipe；D figures are the schematic diagram that inner sleeve presses downwards；E figures are inner sleeve
Pipe is pressed onto bottom and completes the schematic diagram for being inserted into sampling probe Aspirate supernatant after original position is filtered again.
Fig. 3 is the Continuous Flow Analysis instrument pipe-line system schematic diagram of Cr VI detection.
Specific implementation mode
The present invention is further described by following specific examples, but does not limit the present invention.
Embodiment 1：The measurement of Cr VI in colorized cigarette paper sample
1) sample pre-treatments：The representative colorized cigarette paper samples of 50g are extracted, sample is cut into 5mm × 5mm's
Fragment, mixing.Then following processing is pressed：
A, 0.20g samples accurately are weighed to be placed in 25mL sample cells, is removed from Continuous Flow Analysis instrument autosampler
Sample injection disc will claim excellent sample feeding pipe to be put into successively on Continuous Flow Analysis instrument sample injection disc, until by 100 in the sample injection disc
All pile sample cell in sample cell position；
B, dipotassium hydrogen phosphate cushioning liquid 20mL is separately added into each sample cell with the liquid-transfering gun of 25mL, then successively
It is inserted into the inner sleeve of the internal filtering sieve plate for having solid phase extraction filler and bottom to carry 0.45 μm of aperture, prevents oscillation extraction process
Middle solution splashes out, and sample disc is put on oscillator after being plugged inner sleeve, is carried out by the oscillation extraction condition that standard method is selected
Oscillation extraction；
C, the inner sleeve of sample cell is pushed after having extracted, the sample solution extracted is allowed to pass through the filtering sieve plate and institute
It states solid phase extraction filler to enter in inner sleeve, then sample disc is placed on the autosampler of Continuous Flow Analysis instrument, from
The sample introduction needle of dynamic injector is only insertd into every time to draw the supernatant by filtering and extracting at the supernatant in inner sleeve, is turned
Enter and is analyzed in Continuous Flow Analysis instrument.
2) complete according to company standard YQ/T 60-2015 (cigarette tipping paper Determination of Hexavalent Chromium continuous flow method) relevant regulations
At the subsequent measurements work of Cr VI in sample.
It is 0.674 μ g/g to measure content of 6-valence Cr ions in colorized cigarette paper sample.
Embodiment 2：The measurement of Cr VI in tipping paper sample
The process in embodiment 1 is repeated, carries out the measurement of Cr VI in tipping paper sample, measuring content of 6-valence Cr ions is
0.563μg/g。
Claims (2)
1. a kind of high-throughput Continuous Flow Analysis method of Cr VI in colorized cigarette paper and tipping paper, which is characterized in that including
Following steps：
A, 0.20g samples accurately are weighed to be placed in 25mL sample cells, sample introduction is removed from Continuous Flow Analysis instrument autosampler
Disk will claim excellent sample feeding pipe to be put into successively on Continuous Flow Analysis instrument sample injection disc, until by 100 samples in the sample injection disc
All pile sample cell in pipe position；
B, it is separately added into dipotassium hydrogen phosphate cushioning liquid 20mL into each sample cell with the liquid-transfering gun of 25mL, is then sequentially inserted into
There is the inner sleeve of the filtering sieve plate of solid phase extraction filler and bottom with 0.45 μm of aperture in inside, prevents molten during oscillation extraction
Liquid splashes out, and sample disc is put on oscillator after being plugged inner sleeve, and the oscillation extraction condition selected by standard method is vibrated
Extraction；
C, the inner sleeve of sample cell is pushed after having extracted, the sample solution that has extracted is allowed to pass through the filtering sieve plate and described solid
Phase extraction stuffing enters in inner sleeve, then sample disc is placed on the autosampler of Continuous Flow Analysis instrument, automatically into
The sample introduction needle of sample device is only insertd at the supernatant in inner sleeve every time to draw the supernatant by filtering and extracting, the company of being transferred to
It is analyzed in continuous Flow Analyzer.
2. high throughput Continuous Flow Analysis method according to claim 1, which is characterized in that carried at the top of the sample cell
Sealing ring, the inner sleeve are inserted into before oscillation extraction in the sealing ring, and extract liquor is then added, and inner sleeve is stuck in sample
The oral area of quality control prevents extract liquor in oscillatory process from splashing out, but the filtering sieve plate of inner sleeve bottom of the tube is not contacted with sample；Sample extracts
Inner sleeve is pushed after taking, extract liquor is just entered by sieve plate filtering in inner sleeve, and autosampler can be directly from inner sleeve
Sample is extracted in pipe to be analyzed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810146844.5A CN108680655A (en) | 2018-02-12 | 2018-02-12 | A kind of high-throughput Continuous Flow Analysis method of Cr VI in colorized cigarette paper and tipping paper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810146844.5A CN108680655A (en) | 2018-02-12 | 2018-02-12 | A kind of high-throughput Continuous Flow Analysis method of Cr VI in colorized cigarette paper and tipping paper |
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| CN108680655A true CN108680655A (en) | 2018-10-19 |
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| CN201810146844.5A Pending CN108680655A (en) | 2018-02-12 | 2018-02-12 | A kind of high-throughput Continuous Flow Analysis method of Cr VI in colorized cigarette paper and tipping paper |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111157517A (en) * | 2020-01-03 | 2020-05-15 | 吉林烟草工业有限责任公司 | Method for detecting hexavalent chromium in cigarette mainstream smoke |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603925A (en) * | 2009-07-23 | 2009-12-16 | 江苏德林环保技术有限公司 | The hyperchannel direction selecting flow-injection quick analysis system for hexavalent chromium water quality |
| CN103185756A (en) * | 2011-12-28 | 2013-07-03 | 中国石油天然气股份有限公司 | Sample pretreatment method for analysis of anions in alkanolamine solution |
-
2018
- 2018-02-12 CN CN201810146844.5A patent/CN108680655A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101603925A (en) * | 2009-07-23 | 2009-12-16 | 江苏德林环保技术有限公司 | The hyperchannel direction selecting flow-injection quick analysis system for hexavalent chromium water quality |
| CN103185756A (en) * | 2011-12-28 | 2013-07-03 | 中国石油天然气股份有限公司 | Sample pretreatment method for analysis of anions in alkanolamine solution |
Non-Patent Citations (1)
| Title |
|---|
| 中国烟草总公司: "《中国烟草总公司企业标准 YQ/T 60-2015 烟用接装纸 六价铬测定 连续流动法》", 6 February 2015 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111157517A (en) * | 2020-01-03 | 2020-05-15 | 吉林烟草工业有限责任公司 | Method for detecting hexavalent chromium in cigarette mainstream smoke |
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Application publication date: 20181019 |
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